CN102839197B - Low-pollution combined production process of wheatgrass microcrystalline cellulose and biomass ethanol - Google Patents
Low-pollution combined production process of wheatgrass microcrystalline cellulose and biomass ethanol Download PDFInfo
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- CN102839197B CN102839197B CN201210325435.4A CN201210325435A CN102839197B CN 102839197 B CN102839197 B CN 102839197B CN 201210325435 A CN201210325435 A CN 201210325435A CN 102839197 B CN102839197 B CN 102839197B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
A low-pollution combined production process of wheatgrass microcrystalline cellulose and biomass ethanol is characterized in that an acid hydrolysis process is adopted to separate crystalline region of wheatgrass cellulose and an alkali treatment process is carried out to remove ash (a wheatgrass raw material has high ash content) so as to prepare cellulose functionalized product-microcrystalline cellulose with higher crystallinity requirement; absolutely most of amorphous regions and a few of crystalline regions of cellulose are hydrolyzed into glucose in the processes and generated glucose is stored in acid hydrolysis waste liquid and alkali treatment waste liquid; and the two waste liquids are mutually neutralized and glucose is converted into biomass ethanol by adopting a biofermentation method. Therefore, the pollution of the waste liquids to the environment is prevented, wastes are changed into valuables, the glucose resources are utilized and efficient utilization of cellulose is realized. In addition, wheatgrass is used as the raw material to produce microcrystalline cellulose and biomass ethanol, so that the shortage problem of timber, cotton and other the production raw materials for microcrystalline cellulose is alleviated, and agricultural waste-wheat straw resource is sufficiently utilized.
Description
Technical field
The invention belongs to natural polymer technical field, be specifically related to the low pollution joint process of a kind of wheatgrass microcrystalline cellulose and biomass ethanol.
Background technology
One of major technique bottleneck that lignocellulose-like biomass resource utilization and recovery energy exist is at present in Mierocrystalline cellulose, to have fine and close crystalline structure, has seriously hindered chemical reagent or biological enzyme to cellulosic accessibility.The 2nd, cellulose degraded Mierocrystalline cellulose efficiency is low, and cost is high, and industrialization is also difficult to realize at present completely.Therefore the technology that, the full thaumatropy of Mierocrystalline cellulose is biomass fuel is also difficult to obtain very big breakthrough at present.
In addition, produce Microcrystalline Cellulose both at home and abroad and be taking timber and cotton as raw material, its production technique has very large shortcoming: the one, and cotton is relative in short supply with resources such as timber, and cost is high, has limited the industrial scale of Microcrystalline Cellulose; And in current production technique, Mierocrystalline cellulose pars amorpha is used as waste after degrading and discharges, and has both polluted environment, has wasted again resource.
Summary of the invention
The object of the present invention is to provide a kind of taking agriculture production waste---wheat straw is raw material, and preparation technology's environmental protection, the low pollution joint process of the wheatgrass microcrystalline cellulose that resource utilization is high and biomass ethanol.
For achieving the above object, the technical solution used in the present invention is:
1) first, it is to stir in 2% ~ 24% hydrochloric acid soln that pure wheat straw Ethanol Method cellulose prods (seeing patent 200910023763.7) is added to mass concentration, the solid-to-liquid ratio of Mierocrystalline cellulose and hydrochloric acid is 1:4 ~ 1:28, at 40 ~ 120 DEG C, be hydrolyzed 30 ~ 150min, separated product is insolubles and acidic solution;
2) insolubles is dispersed in water to make insolubles quality concentration be 5% ~ 40%, and add the NaOH of insolubles quality 2% ~ 18% to process 20 ~ 90min at 20 ~ 100 DEG C, filter and obtain insolubles and basic solution afterwards, washing insolubles obtains the cellulose prods of high-crystallinity;
3) warm air drying with 35 ~ 125 DEG C by the cellulose prods of high-crystallinity, then drying products is pulverized, and screened with 120 mesh sieves, be Microcrystalline Cellulose product by the part of sieve aperture, can not repeat to pulverize and sieve by sieve aperture part, until all pass through sieve aperture;
4) by acidic solution and step 2 in step 1)) in basic solution be mixed to get mixed waste liquor, and then to regulate the pH value of this mixed waste liquor with the hydrochloric acid soln that mass concentration is 1% ~ 28% be 5.0;
5) by this mixed waste liquor at 0.1 ~ 0.5MPa, under 100 ~ 165 DEG C of conditions, carry out sterilising treatment 30min;
6) in mixed waste liquor, add the yeast saccharomyces cerevisiae after 3%～24% activation of mixed waste liquor volume to ferment, leavening temperature is 15～60 DEG C, and fermentation time is 12～108h, and the glucose that can transform in waste liquid is ethanol;
7) fermented liquid is carried out to air distillation, collect the cut in 77 ~ 79 DEG C of temperature ranges, can obtain volumetric concentration and be 93%～95% biomass ethanol.
The present invention is directed to constructional feature and the performance difference of Mierocrystalline cellulose crystallizing field and pars amorpha, take different treatment, respectively utilize thinking, by acid hydrolysis and alkaline purification technical point from crystallizing field for the preparation of MCC, pars amorpha is dissolved in respectively in acid hydrolysis and alkaline purification waste liquid after being hydrolyzed to glucose, the glucose that utilizes two kinds of waste liquids mutually to neutralize and adopt the method for biological fermentation to transform is wherein ethanol, has dissolved this two technical barriers.
It is glucose that purer wheat straw Ethanol Method Mierocrystalline cellulose is adopted to acid hydrolysis technology its pars amorpha of degrading, and retains crystallizing field, and through alkaline purification except deashing (wheat straw raw material ash content is larger); Finally prepare Microcrystalline Cellulose product by dry, disintegrating process.In acid hydrolysis and alkaline purification process, most Mierocrystalline celluloses pars amorpha and a small amount of crystallizing field are degraded to glucose and are dissolved in acid hydrolysis and alkaline purification waste liquid.Utilize two kinds of waste liquids mutually to neutralize, and the glucose that the method that adopts biological fermentation transforms is wherein biomass ethanol, both reduce the pollution of waste liquid to environment, can greatly improve again the utilization ratio of cellulose resource, realized the low pollution coproduction of wheatgrass microcrystalline cellulose and biomass ethanol.
Embodiment
Embodiment 1:
1) first, it is to stir in 10% hydrochloric acid soln that pure wheat straw Ethanol Method cellulose prods (seeing patent 200910023763.7) is added to mass concentration, the solid-to-liquid ratio of Mierocrystalline cellulose and hydrochloric acid is 1:12, at 40 DEG C, is hydrolyzed 150min, and separated product is insolubles and acidic solution;
2) insolubles is dispersed in water to make insolubles quality concentration be 30%, and adds the NaOH of insolubles quality 15% to process 90min at 20 DEG C, filter and obtain insolubles and basic solution afterwards, washing insolubles obtains the cellulose prods of high-crystallinity;
3) warm air drying with 100 DEG C by the cellulose prods of high-crystallinity, then drying products is pulverized, and screened with 120 mesh sieves, be Microcrystalline Cellulose product by the part of sieve aperture, can not repeat to pulverize and sieve by sieve aperture part, until all pass through sieve aperture;
4) by acidic solution and step 2 in step 1)) in basic solution be mixed to get mixed waste liquor, and then to regulate the pH value of this mixed waste liquor with the hydrochloric acid soln that mass concentration is 1% be 5.0;
5) by this mixed waste liquor at 0.1MPa, under 165 DEG C of conditions, carry out sterilising treatment 30min;
6) in mixed waste liquor, add the yeast saccharomyces cerevisiae after 24% activation of mixed waste liquor volume to ferment, leavening temperature is 15 DEG C, and fermentation time is 108h, and the glucose that can transform in waste liquid is ethanol;
7) fermented liquid is carried out to air distillation, collect the cut in 77 ~ 79 DEG C of temperature ranges, can obtain volumetric concentration and be 93%～95% biomass ethanol.
Embodiment 2:
1) first, it is to stir in 2% hydrochloric acid soln that pure wheat straw Ethanol Method cellulose prods (seeing patent 200910023763.7) is added to mass concentration, the solid-to-liquid ratio of Mierocrystalline cellulose and hydrochloric acid is 1:28, at 80 DEG C, is hydrolyzed 90min, and separated product is insolubles and acidic solution;
2) insolubles is dispersed in water to make insolubles quality concentration be 10%, and adds the NaOH of insolubles quality 12% to process 20min at 100 DEG C, filter and obtain insolubles and basic solution afterwards, washing insolubles obtains the cellulose prods of high-crystallinity;
3) warm air drying with 35 DEG C by the cellulose prods of high-crystallinity, then drying products is pulverized, and screened with 120 mesh sieves, be Microcrystalline Cellulose product by the part of sieve aperture, can not repeat to pulverize and sieve by sieve aperture part, until all pass through sieve aperture;
4) by acidic solution and step 2 in step 1)) in basic solution be mixed to get mixed waste liquor, and then to regulate the pH value of this mixed waste liquor with the hydrochloric acid soln that mass concentration is 15% be 5.0;
5) by this mixed waste liquor at 0.3MPa, under 130 DEG C of conditions, carry out sterilising treatment 30min;
6) in mixed waste liquor, add the yeast saccharomyces cerevisiae after 20% activation of mixed waste liquor volume to ferment, leavening temperature is 20 DEG C, and fermentation time is 90h, and the glucose that can transform in waste liquid is ethanol;
7) fermented liquid is carried out to air distillation, collect the cut in 77 ~ 79 DEG C of temperature ranges, can obtain volumetric concentration and be 93%～95% biomass ethanol.
Embodiment 3:
1) first, it is to stir in 24% hydrochloric acid soln that pure wheat straw Ethanol Method cellulose prods (seeing patent 200910023763.7) is added to mass concentration, the solid-to-liquid ratio of Mierocrystalline cellulose and hydrochloric acid is 1:4, at 60 DEG C, is hydrolyzed 120min, and separated product is insolubles and acidic solution;
2) insolubles is dispersed in water to make insolubles quality concentration be 40%, and adds the NaOH of insolubles quality 18% to process 50min at 50 DEG C, filter and obtain insolubles and basic solution afterwards, washing insolubles obtains the cellulose prods of high-crystallinity;
3) warm air drying with 50 DEG C by the cellulose prods of high-crystallinity, then drying products is pulverized, and screened with 120 mesh sieves, be Microcrystalline Cellulose product by the part of sieve aperture, can not repeat to pulverize and sieve by sieve aperture part, until all pass through sieve aperture;
4) by acidic solution and step 2 in step 1)) in basic solution be mixed to get mixed waste liquor, and then to regulate the pH value of this mixed waste liquor with the hydrochloric acid soln that mass concentration is 20% be 5.0;
5) by this mixed waste liquor at 0.5MPa, under 100 DEG C of conditions, carry out sterilising treatment 30min;
6) in mixed waste liquor, add the yeast saccharomyces cerevisiae after 15% activation of mixed waste liquor volume to ferment, leavening temperature is 30 DEG C, and fermentation time is 70h, and the glucose that can transform in waste liquid is ethanol;
7) fermented liquid is carried out to air distillation, collect the cut in 77 ~ 79 DEG C of temperature ranges, can obtain volumetric concentration and be 93%～95% biomass ethanol.
Embodiment 4:
1) first, it is to stir in 6% hydrochloric acid soln that pure wheat straw Ethanol Method cellulose prods (seeing patent 200910023763.7) is added to mass concentration, the solid-to-liquid ratio of Mierocrystalline cellulose and hydrochloric acid is 1:24, at 100 DEG C, is hydrolyzed 60min, and separated product is insolubles and acidic solution;
2) insolubles is dispersed in water to make insolubles quality concentration be 20%, and adds the NaOH of insolubles quality 2% to process 30min at 80 DEG C, filter and obtain insolubles and basic solution afterwards, washing insolubles obtains the cellulose prods of high-crystallinity;
3) warm air drying with 80 DEG C by the cellulose prods of high-crystallinity, then drying products is pulverized, and screened with 120 mesh sieves, be Microcrystalline Cellulose product by the part of sieve aperture, can not repeat to pulverize and sieve by sieve aperture part, until all pass through sieve aperture;
4) by acidic solution and step 2 in step 1)) in basic solution be mixed to get mixed waste liquor, and then to regulate the pH value of this mixed waste liquor with the hydrochloric acid soln that mass concentration is 28% be 5.0;
5) by this mixed waste liquor at 0.2MPa, under 150 DEG C of conditions, carry out sterilising treatment 30min;
6) in mixed waste liquor, add the yeast saccharomyces cerevisiae after 10% activation of mixed waste liquor volume to ferment, leavening temperature is 40 DEG C, and fermentation time is 50h, and the glucose that can transform in waste liquid is ethanol;
7) fermented liquid is carried out to air distillation, collect the cut in 77 ~ 79 DEG C of temperature ranges, can obtain volumetric concentration and be 93%～95% biomass ethanol.
Embodiment 5:
1) first, it is to stir in 15% hydrochloric acid soln that pure wheat straw Ethanol Method cellulose prods (seeing patent 200910023763.7) is added to mass concentration, the solid-to-liquid ratio of Mierocrystalline cellulose and hydrochloric acid is 1:20, at 120 DEG C, is hydrolyzed 50min, and separated product is insolubles and acidic solution;
2) insolubles is dispersed in water to make insolubles quality concentration be 5%, and adds the NaOH of insolubles quality 6% to process 60min at 60 DEG C, filter and obtain insolubles and basic solution afterwards, washing insolubles obtains the cellulose prods of high-crystallinity;
3) warm air drying with 110 DEG C by the cellulose prods of high-crystallinity, then drying products is pulverized, and screened with 120 mesh sieves, be Microcrystalline Cellulose product by the part of sieve aperture, can not repeat to pulverize and sieve by sieve aperture part, until all pass through sieve aperture;
4) by acidic solution and step 2 in step 1)) in basic solution be mixed to get mixed waste liquor, and then to regulate the pH value of this mixed waste liquor with the hydrochloric acid soln that mass concentration is 5% be 5.0;
5) by this mixed waste liquor at 0.4MPa, under 120 DEG C of conditions, carry out sterilising treatment 30min;
6) in mixed waste liquor, add the yeast saccharomyces cerevisiae after 6% activation of mixed waste liquor volume to ferment, leavening temperature is 50 DEG C, and fermentation time is 30h, and the glucose that can transform in waste liquid is ethanol;
7) fermented liquid is carried out to air distillation, collect the cut in 77 ~ 79 DEG C of temperature ranges, can obtain volumetric concentration and be 93%～95% biomass ethanol.
Embodiment 6:
1) first, it is to stir in 20% hydrochloric acid soln that pure wheat straw Ethanol Method cellulose prods (seeing patent 200910023763.7) is added to mass concentration, the solid-to-liquid ratio of Mierocrystalline cellulose and hydrochloric acid is 1:8, at 90 DEG C, is hydrolyzed 100min, and separated product is insolubles and acidic solution;
2) insolubles is dispersed in water to make insolubles quality concentration be 25%, and adds the NaOH of insolubles quality 10% to process 70min at 40 DEG C, filter and obtain insolubles and basic solution afterwards, washing insolubles obtains the cellulose prods of high-crystallinity;
3) warm air drying with 125 DEG C by the cellulose prods of high-crystallinity, then drying products is pulverized, and screened with 120 mesh sieves, be Microcrystalline Cellulose product by the part of sieve aperture, can not repeat to pulverize and sieve by sieve aperture part, until all pass through sieve aperture;
4) by acidic solution and step 2 in step 1)) in basic solution be mixed to get mixed waste liquor, and then to regulate the pH value of this mixed waste liquor with the hydrochloric acid soln that mass concentration is 10% be 5.0;
5) by this mixed waste liquor at 0.3MPa, under 110 DEG C of conditions, carry out sterilising treatment 30min;
6) in mixed waste liquor, add the yeast saccharomyces cerevisiae after 3% activation of mixed waste liquor volume to ferment, leavening temperature is 60 DEG C, and fermentation time is 12h, and the glucose that can transform in waste liquid is ethanol;
7) fermented liquid is carried out to air distillation, collect the cut in 77 ~ 79 DEG C of temperature ranges, can obtain volumetric concentration and be 93%～95% biomass ethanol.
The present invention requires high cellulose functionalized product---Microcrystalline Cellulose by the crystallizing field that separates wheatgrass cellulose for the preparation of degree of crystallinity, overwhelming majority Mierocrystalline cellulose pars amorpha and a small amount of crystallizing field are present in after hydrolysis and saccharification in acid hydrolysis and alkaline purification waste liquid in acid hydrolysis and alkaline purification process, two kinds of waste liquids are neutralized mutually and for fermentation of biomass ethanol, both prevented the pollution of waste liquid to environment, more turn waste into wealth, utilize glucose resource wherein, cellulosic resource utilization and energy comprehensive utilization are realized, for agriculture stalk total composition, full structure, multi-product coproduction efficient technique of rainwater utilization theory provides new thinking.Finally, taking wheat straw as raw material production Microcrystalline Cellulose with biomass ethanol, both the problem in short supply of having alleviated the Microcrystalline Cellulose such as timber, cotton raw materials for production, takes full advantage of again agricultural wastes wheat straw resource, has higher expection economic benefit and social benefit.
Claims (1)
1. the low pollution joint process of wheatgrass microcrystalline cellulose and biomass ethanol, is characterized in that:
1) first, it is to stir in 2% ~ 24% hydrochloric acid soln that pure wheat straw Ethanol Method cellulose prods is added to mass concentration, the solid-to-liquid ratio of Mierocrystalline cellulose and hydrochloric acid is 1:4 ~ 1:28, at 40 ~ 120 DEG C, is hydrolyzed 30 ~ 150min, and separated product is insolubles and acidic solution;
2) insolubles is dispersed in water to make insolubles quality concentration be 5% ~ 40%, and add the NaOH of insolubles quality 2% ~ 18% to process 20 ~ 90min at 20 ~ 100 DEG C, filter and obtain insolubles and basic solution afterwards, washing insolubles obtains the cellulose prods of high-crystallinity;
3) warm air drying with 35 ~ 125 DEG C by the cellulose prods of high-crystallinity, then drying products is pulverized, and screened with 120 mesh sieves, be Microcrystalline Cellulose product by the part of sieve aperture, can not repeat to pulverize and sieve by sieve aperture part, until all pass through sieve aperture;
4) by acidic solution and step 2 in step 1)) in basic solution be mixed to get mixed waste liquor, and then to regulate the pH value of this mixed waste liquor with the hydrochloric acid soln that mass concentration is 1% ~ 28% be 5.0;
5) by this mixed waste liquor at 0.1 ~ 0.5MPa, under 100 ~ 165 DEG C of conditions, carry out sterilising treatment 30min;
6) in mixed waste liquor, add the yeast saccharomyces cerevisiae after 3%～24% activation of mixed waste liquor volume to ferment, leavening temperature is 15～60 DEG C, and fermentation time is 12～108h, and the glucose that can transform in waste liquid is ethanol;
7) fermented liquid is carried out to air distillation, collect the cut in 77 ~ 79 DEG C of temperature ranges, can obtain volumetric concentration and be 93%～95% biomass ethanol.
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| CN107686106A (en) * | 2017-08-22 | 2018-02-13 | 杨子中 | The method that biomass graphene is prepared with wheat straw extraction cellulose |
| CN115874481A (en) * | 2022-11-24 | 2023-03-31 | 新疆金色果园农林科技有限公司 | Microcrystalline cellulose extracted from grape skin residues and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101649569A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Process for preparing low-pollution wheatgrass microcrystalline cellulose |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101649569A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Process for preparing low-pollution wheatgrass microcrystalline cellulose |
Non-Patent Citations (2)
| Title |
|---|
| 木质纤维素稀酸水解液乙醇发酵的新方法;钱名字等;《太阳能学报》;20060630;第27卷(第6期);618-619 * |
| 钱名字等.木质纤维素稀酸水解液乙醇发酵的新方法.《太阳能学报》.2006,第27卷(第6期),618-619. |
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